Apparatus for producing antira



Feb. 1, 1938. Y I c. c. WHlTTlER 2,106,781

APPARATUS FOR PRODUCING ANTIRACHITIC PRODUCTS Filed July 5, 1955 1 .Z'12 yen for I Patented Feb. 1, 1938 PATENT OFFICE APPARATUS FOR raonuomean'rmsom'nc raonuc'rs came; 0. Whittier, Chicago, in, lalllnor toNutritio in Research Laboratories, Inc., Chicago,

a corporation of Delaware Application July s. 1935. Serial No. aassi v 2Claim.

This invention relates to method and apparatus for antirachiticallyactivating ergosterol and related substances in the commercialproduction of vitamin D.

6 The main objects of this invention are to provide an improved form ofapparatus of the type described inmy co-pending application for LettersPatent, Serial No. 711,539, filed February 16, 1934, with particularreference to structural im- 10 provements for manufacturing antirachiticproducts on a commercial scale; without exposing either the raw materialor finished product to contact with or proximity to a charged electrode,and to carry out the process at such low vacuum 18 that the flow ofcurrent will be silent.

Certain structural features, shown but not claimed herein, are claimedin my co-pending apglliation Serial No. 29,882 filed of even date here-A specific embodiment of this invention is illustrated in theaccompanying drawing in which: Figure 1 is a vertical section of thecomplete apparatus, the vacuum pump and source of electric current beingindicated by their connection a fittings and line wires respectively.

Fig. 2 is a transverse section takenon the line 2-2 of Fig. 1 andshowing a detail of the gate in the condenser housing to permit easyremoval of the tube.

a In the form shown in the drawing, the apparatus comprises a vacuumtube preferably formed of glass or other dielectric material and made upof a plurality of communicating sections or 1 chambers in all of which avacuum is maintained a by means oi a vacuum pump which may be of anysuitable commercial forin and is accordingly represented in the drawingby one of its connecting fittings i with which the main tube isconnectedas for example, bythe conically a ground joint I.

The processing tube comprises an upright portion 3 which forms the"treatment chamber 4.

Below the treatment chamber 4 is a bulbous va-.

porizing chamber or flash 1. Appropriate heata ing means indicated asthe flame from a burner lubricated, allows the receptacle it to berotated on the joint I! to control the rate at which the raw material,usually ergosterol, is fed to the flask I. 4

The-upper end of the tubular portion 3 is en- 5 larged to form a bulbIt. The bulb l-l has a somewhat enlarged tubular branch ii whichconnects with larger globular member l6 which, together with a dependingbranch It forms an expansion and condensing chamber ll. The vac- 10 uumpump communicates with the interior of the condenser ll through a tubei9/which extends down to the lower portion of the branch is andhastapered and ground slip joints at 2 and '20 where it connects with thefitting i and the 1 I outlet throat II of the condenser chamber.

The condenser I1 is surrounded by a jacket or housing 22 which supportsa suitable refrigerant, such for example, as solid carbondioxide or dryice filling the space 23, and in contact with the walls of the chamberII.

The electrical leads 24 are connected with a source of electric currentwhich may be either 'direct or alternating. In practice, I usealternating current of 20,000 volts and 10 milliam- 25 Y pers obtainedfrom the secondary circuit-of a I have specified herein certainelectrical curv rent characteristics that I have used extensively in thecommercial production of antirachitic products, that measure up to themost exacting tests 'of potency, including American Pharmacopoeiastandards, and the international stand- 40 ards established by theLeague of Nations and defined in its publication Ofllcial No. C. H. 1056(1) Geneva, 1931 (London June 23, 1931) and in no instance has theproduct exhibited any of the 'undesirable characteristics, such astachosterol,

toxisterol and others, that have been ascribed to overexposure ofergosterol or alimentary products to ultra-violet light. The low vacuumof one-half millimeter to one millimeter of mercury head that I maintainin order to control the fiow of vaporized ergosterol at the desiredrate, at the voltages specified, and the absence of any metallic gas inthe system, preclude thev production of any ultra-violet light in myprocess. I 'urthermore, I have provided tortuous branch connec-- tions26 and 21 to the opposite ends of my treatment chamber 4 and placed theelectric terminals." and 29 so as to be exposed to the contents of thetube but in remote positions in these branches so that by no chance canstraight line discharges at these terminals reach the zone occupied bythe vapors being treated. The .aotivating electrical influence is asilent discharge or flow of electricity of which the ergosterol vapor isthe conducting medium.

In operation, after the device is set up as shown in Fig. 1, the vacuumpump is operated to maintain a vacuum equivalent to one-half to onemillimeter of mercury column which is main tained by continuousoperation of the vacuum pump throughout the process.

A supply of the raw material to .be treated, usually ergosterol, isplaced in the receptacle I0 and after the desired vacuum is attained,the receptacle I0 is gradually rotated to discharge a fine stream of thepowdered ergosterol through the inlet tube 9 to the flask 1 where it isvaporized by the heat of the burner 8 whose flame is played upon thewalls of the flask "I in such a way as to avoid excessive heating andmaintain a uniform rate of evaporation of the ergosterol.

The vapor oi ergosterol rises through the chamber 4 where it issubjected to the electrical infiuence produced by the current from theleads 24. The expression electrical influence is intended to describeany and all electrical conditions that are responsible for theantirachitic activation of the vapor as it traverses the space 4.

The term ergosterol is intended to include ergosterol per so, as well assubstances related to it, such as lipins, sterols, cholesterol,zoosteroi and the like.

The branch l8 and exhaust tube l9 are extended to sufflcient length toavoid any escape of the substance treated into the exhaust piping orpump. The finished product may be removed from the condenser by scrapingor brushing it ofl! from the condenser walls or by dissolving it inether.

Although but one specific embodiment of this invention is herein shownand described, it is to be understood that details as set forth may bealtered or omitted without departing from the spirit of the invention asdefined by the following claims.

Iclaim:

1. In apparatus for antirachitic activation of alimentary substances, avacuum tube having means to maintain a vacuum therein, a. supplychamber, a vaporizing chamber, a treatment chamber, a condensing chambercommunicating with each other, said tube having branches incommunication with opposite ends respectively of said treatment chamberand a source of electric current having terminals exposed to thecontents of said tube .for causing an electric current to flow throughthe vapor in said treatment chamber, said terminals being each locatedin said branches remote from said treatment chamber, and in suchdisposition as to exclude straight line discharges from one terminal tothe other.

2. In apparatus for antirachitic activation of alimentary substances, avacuum tube having means to maintain a vacuum therein, a 'supplychamber, a vaporizing chamber, a treatment chamber, and a condensingchamber communi- 5 eating with each other, said tube having tortuousbranches in communication with opposite ends respectively of saidtreatment chamber, and a source of electric current having terminals forcausing an electric current to flow through the vapor in said treatmentchamber, said terminals being exposed to the contents of said tube andeach located respectively in said branches remote from said treatmentchamber.

CHARLES C. Wm.

